Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 23284734 | HCID 23284734 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 23284738 | HCID 23284738 | 74.8% |
Reaction Steps
6,7-Difluoro-1-(4-fluoro-3-hydroxyphenyl)-8-methyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (403 mg) and an aqueous solution (about 40%; 2.0 g) of methylamine were added to pyridine (2.0 g), and the mixture was stirred at 60° C. for 6 days. The reaction mixture was concentrated under reduced pressure. A process of adding ethanol (5 ml) to the residue and then concentrating the mixture under reduced pressure was conducted 3 times repeatedly. Ethanol (2 ml) was added to the resultant residue, and deposits were collected by filtration and washed with ethanol and diisopropyl ether in that order to obtain the title compound (311 mg) as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06136823 |
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| Source dataset | uspto-grants-2000_10 |
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| ORD ID | ord-9f264bad32044a80a3bb60640070b585 |
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| Source note | uspto-grants-2000_10 |
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